Sodium sulfate decahydrate → HCID 59334545, compound

HRID 1639880Notes

Reaction equation

HRID 1639880 reaction equation
[H-].[Al+3].[Li+].[H-].[H-].[H-].[CH3:7][C:8]1[N:22]=[C:11]2[CH:12]=[CH:13][CH:14]=[C:15]([CH:16]3[CH2:18][CH:17]3[CH:19]=[N:20]O)[N:10]2[N:9]=1.O.O.O.O.O.O.O.O.O.O.S([O-])([O-])(=O)=O.[Na+].[Na+]>O1CCCC1>[CH3:7][C:8]1[N:22]=[C:11]2[CH:12]=[CH:13][CH:14]=[C:15]([CH:16]3[CH2:18][CH:17]3[CH2:19][NH2:20])[N:10]2[N:9]=1

Participants

5

Reactant 3

HCID 62649Sodium sulfate decahydrateHCID 21226445Aluminium lithium hydrideHCID 72257851HCID 72257851, compound

Product 1

HCID 59334545HCID 59334545, compound

Reagents, catalysts & solvents 1

HCID 8028TetrahydrofuranSolvent

Procedure

To a suspension of lithium aluminum hydride (141 mg, 3.70 mmol) in tetrahydrofuran (10 mL) was added 2-(2-methyl[1,2,4]triazolo[1,5-a]pyridin-5-yl)cyclopropanecarbaldehyde oxime (200 mg, 0.925 mmol) obtained in Reference Example 112 at room temperature, and the mixture was stirred at room temperature for 2 hr, and at 60° C. for 2 hr. Sodium sulfate decahydrate was added under ice-cooling, and the mixture was filtered through celite. The filtrate was concentrated under reduced pressure to give 1-[2-(2-methyl[1,2,4]triazolo[1,5-a]pyridin-5-yl)cyclopropyl]methanamine as a crudely purified product.

Workup

  1. customobtained in Reference Example 112 at room temperature
  2. waitat 60° C. for 2 hr
  3. temperaturecooling
  4. filtrationthe mixture was filtered through celite
  5. concentrationThe filtrate was concentrated under reduced pressure

Sources & evidence

ORD record
ord-7127185ac81046feb7203c53de828525
Source dataset
uspto-grants-2012_02
Patent number
US08110585B2

Reaction notes

Loading…